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1.
Szabolcs Szarka Vien Nguyen Laszlo Prokai Katalin Prokai-Tatrai 《Analytical and bioanalytical chemistry》2013,405(10):3399-3406
We show here that baseline separation of dansylated estrone, 17β-estradiol, and 17α-estradiol can be done, contrary to previous reports, within a short run time on a single RP-LC analytical column packed with particles bonded with phenyl-hexyl stationary phase. The chromatographic method coupled with isotope dilution tandem MS offers a simple assay enabling the simultaneous analysis of these analytes. The method employs 13C-labeled estrogens as internal standards to eliminate potential matrix effects arising from the use of deuterated estrogens. The assay also offers adequate accuracy and sensitivity to be useful for biological samples. The practical applicability of the validated method is demonstrated by the quantitative analyses of in vivo samples obtained from rats treated with Premarin®. Figure
Quantification of estrogens from rat samples by LC–MS/MS 相似文献
2.
GC–MS Studies of Thiophenes in the Supercritical Fluid CO2 and Solvent Extracts of Tagetes patula L.
Szabolcs Szarka István Gyurján Miklós László Éva Héthelyi Inna N. Kuzovkina Éva Lemberkovics Éva Szőke 《Chromatographia》2010,71(11-12):1039-1047
The intact plant parts and genetically modified hairy root clone #TpA6 of Tagetes patula were extracted with supercritical fluid CO2 extraction (SFE) and a conventional solvent extraction. SFE optimization included the variation of fluid CO2 pressure, dynamic time, and the addition of methanol modifier co-solvent. The four characteristic thiophene metabolites, 5-(3-buten-1-ynyl)-2,2′-bithienyl (BBT), 2,2′:5′,2″-terthiophene (α-T), 5-(4-acetoxy-1-butynyl)-2,2′-bithienyl (BBTOAc), and 5-(3,4-diacetoxy-1-butynyl)-2,2′-bithienyl [BBT(OAc)2], were analysed by GC–MS. The proposed SFE method allowed the selective extraction of thiophenes in 60 min dynamic time with supercritical CO2 without modifier co-solvent, at 30 MPa and 40 °C. The SFE and the reference solvent extraction yielded similar results. The SFE of intact roots and flowers yielded 717 ± 31.3 and 480 ± 26.6 μg g?1 α-T, respectively, while the leaves did not contain considerable amounts of thiophenes. Remarkable amounts of BBT, BBTOAc, and BBT(OAc)2 were characteristic of the SFE of hairy root cultures. 相似文献
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4.
Steroidal 17-hydroxamic acid derivatives were synthesized in high yields in palladium-catalysed carbonylation reaction of 17-iodo-androst-16-ene derivatives under mild reaction conditions. 相似文献
5.
Gas and liquid chromatography coupled with mass spectrometry was applied to solve difficulties and reinvestigate the serious matrix problems affecting analysis of the active compounds in Euphrasia rostkoviana Hayne. The main groups of compounds were obtained by extracting the herb stepwise with n-hexane, chloroform, ethyl acetate and methanol. Polyamide column chromatography facilitated further separation. Phenolic/flavonoid- and terpenoid-type molecules were studied by GC–MS, HPLC and LC–MS–MS. The β-sitosterol content of the herb was determined by gas chromatography with flame ionisation detection (GC-FID). Caffeic acid, chlorogenic acid, coumaric acid and flavonoid glycosides of apigenin, luteolin, rhamnetine (hexoside), kaempferol (both hexoside and rutinoside) and quercetin (rutinoside) were identified in the fractions of the methanolic extract. 相似文献
6.
Chip‐based nanoelectrospray ionization with Fourier transform mass spectrometric detection to screen for local anesthetics intended to mask limb sore in walking horses 下载免费PDF全文
We report a high‐throughput chip‐based nanoelectrospray ionization method coupled with Fourier transform mass spectrometry to screen for local anesthetics in samples collected by swabbing. These drugs have been used to mask pain on the limbs of walking horses after forbidden practices of soring or physical abuse. Optimized for lidocaine, the method afforded sub‐ppm mass accuracy for nine local anesthetics included in the study. From doped cotton swabs, two third and all of the analytes were detected after adding 10 ng and 100 ng of each drug, respectively. Benzocaine and/or lidocaine were found on positive swab samples collected during walking horse competitions. Copyright © 2015 John Wiley & Sons, Ltd. 相似文献
7.
J. Orbán Kinga Pozsonyi Krisztina Szarka Szilvia Barkó Emőke Bódis D. Lőrinczy 《Journal of Thermal Analysis and Calorimetry》2006,84(3):619-623
The thermodynamic properties of the ADP- and ATP-actin filaments were
compared by the method of differential scanning calorimetry. The lower melting
point for the ADP-F-actin filament (58.4 vs. 64.5°C for ATP-F-actin) indicated
that compared to the ATP-actin filaments its structure was less resistant
to heat denaturation. The detailed thermodynamic characterisation of the proteins
was carried out by the analysis of the calorimetric enthalpy, the entropy
and the free enthalpy changes. All of the determined parameters gave lower
values to the ADP-actin filaments than to the ATP-actin filaments. The calculated
values of the activation energy also demonstrated that compared to the ADP-F-actin
the ATP-F-actin was thermodynamically more resistant to the denaturing effect
of heat.
Based on all of this information we have concluded that the actin
filament prepared from ADP containing magnesium saturated actin monomers at
pH 8.0 is thermodynamically less stable than the ones obtained from ATP-actin
monomers. 相似文献
8.
Somogyi B Lakos Z Szarka A Nyitrai M 《Journal of photochemistry and photobiology. B, Biology》2000,59(1-3):26-32
The temperature profile of the normalized fluorescence resonance energy transfer efficiency is capable of monitoring the relative change of flexibility and/or conformational state of macromolecules [Biochemistry 23 (1984) 3403]. The method described earlier for one donor-one acceptor systems is extended to multiple fluorophore systems when the energy transfer occurs between either one donor-m acceptors, or n donors-one acceptor or n donors-m acceptors (where n and m are integer values). It is shown that the normalized energy transfer efficiency obtained for systems containing multiple labels is a linear combination of the normalized transfer efficiency assigned to individual donor-acceptor pairs of the system, thus its temperature profile is capable of monitoring the change of intramolecular flexibility and/or conformational state. 相似文献
9.
Daruhzi gnes E. Szarka Szabolcs Hthelyi va Simndi Bla Gyurjn Istvn Lszl Mikls Szke va Lemberkovics va 《Chromatographia》2008,68(1):71-76
A GC-MS method has been developed for the qualitative analysis of sterol and triterpene (terpenoid) constituents of Ononis spinosa L. (spiny restharrow) root without derivatization. β-Sitosterol, campesterol, stigmasterol, stigmastan-3,5-diene sterol compounds and the triterpene derivatives β-amyrin and α-onocerin were identified. A validated GC-FID quantitative method was developed for measuring β-sitosterol, the main sterol component, in various extracts of this plant, obtained with organic solvents and by supercritical fluid extraction. The extracts were cleaned by saponifying and then the β-sitosterol was quantified in the non-saponifiable fractions by GC-FID with an internal standard. In addition, the relative concentrations of the other terpenoids were also determined. The β-sitosterol content in the non-saponifiable solvent extraction fractions was 0.19–5.5%, that of the supercritical fractions were 4.8–9.2%, depending on the experimental conditions. The hexane and the pilot scale SFE extracts were considered as main sources of terpenoids (71.8%; 93.3%, respectively). 相似文献
10.
Szarka Sz. Hthelyi . Lemberkovics . Kuzovkina I. N. Bnyai P. Szke . 《Chromatographia》2006,63(13):S67-S73
The production and the composition of the compounds (mono-, sesquiterpenes and acetylenic thiophenes) obtained by the steam distillation of Tagetes patula L. have been investigated. The volatile oil was produced by steam distillation. GC was carried out on three types of stationary phase using flame ionization and mass selective detection. Percentage data were calculated by the area normalization method with very good repeatability (RSD below 5%). Oils from flower-heads were rich in β-caryophyllene (53.5%) and the leaves contained terpinolene in high concentration (21.1%). The main volatile component of the hairy roots and intact roots was 5-(3-buten-1-ynyl)-2,2'-bithienyl (BBT) yielding 28.5% and 44.0% in the oils. Three new minor constituents were identified as α-gurjunene, β-caryophyllene and (E)-β-farnesene. A flash chromatographic method was developed for the isolation of thiophenes from a solvent extract of intact roots. The collected fractions were screened by TLC and analyzed by GC-MS. Three thiophene fractions were obtained containing BBT, 5-(4-acetoxy-1-butynyl)-2,2'-bithienyl (BBTOAc) and 5-(4-hydroxy-1-butynyl)-2,2'-bithienyl (BBTOH). 相似文献